CN108046305A - A kind of composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment and preparation method thereof - Google Patents
A kind of composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment and preparation method thereof Download PDFInfo
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- CN108046305A CN108046305A CN201711005750.8A CN201711005750A CN108046305A CN 108046305 A CN108046305 A CN 108046305A CN 201711005750 A CN201711005750 A CN 201711005750A CN 108046305 A CN108046305 A CN 108046305A
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- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/288—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment, the ionic valence condition of the Doped ions M is 2 and at least two kinds, according to molar ratio Ce3+∶MAlways=2 (1 x): 3x, wherein 0 ＜ x≤0.1.In addition, also disclose the composite mixed type γ~Ce of above-mentioned nanoscale low price ion2S3The preparation method of red pigment.The composite mixed low price ion of the present invention enters γ~Ce2S3In lattice, by replacing Ce3+It ion and fills up cation vacancy present in lattice and realizes doping, effectively stabilize γ~Ce2S3Lattice greatly improves the high-temperature stability of pigment, so as to be greatly expanded its application field under the high temperature conditions.Preparation method of the present invention is simple for process easy to operate, and influence factor is easy to control, and production cost is low, contributes to promotion and application.
Description
Technical field
The present invention relates to inorganic pigment technical field more particularly to a kind of ion doping type γ~Ce2S3Red pigment and its
Preparation method.
Background technology
γ~Ce2S3Pigment is in large red, in colour-stable, strong covering power, ultraviolet light resistant, safe and non-toxic, it has also become take
For the first choice of toxic cadmium-selenium red pigment, had a wide range of applications in fields such as plastics, rubber, high-grade paints.However, γ~Ce2S3
Pigment can only use at a temperature of less than 350 DEG C, more than the temperature will decompose rapidly lose it is red, so as to affect it in high temperature
Under application.
In order to improve γ~Ce2S3High-temperature stability, the prior art wrapped mainly using technique for packing on colorant surface
One or more layers transparent high-temperature stability material is covered, it is SiO to study at present more2、ZrSiO4And ZrO2Coated γ~
Ce2S3Colorant, can be by γ~Ce2S3High-temperature stability improve to 550 DEG C.But due to γ~Ce2S3Belong to a cube Th3P4
Type structure, there are cation vacancy in lattice, room forms the S of a distortion in cubic crystal structure4Four sides body hole, from
And cause γ~Ce2S3Crystalline structure is very unstable, easily takes a turn for the worse under high temperature action and is changed into β phases, red so as to lose
Color.Therefore, only by simple package cannot inherently solve the problems, such as crystal structure stablize, although at present also have using from
The mode of son doping realizes stable lattice, although the study found that single ion doping can realize stable lattice, but easily make
Obtain γ~Ce2S3The electronic transition energy of pigment f → d changes, and absorption spectrum changes, bright red so as to cause no longer showing
Color.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of composite mixed type γ of nanoscale low price ion
~Ce2S3Red pigment, in a manner that low price ion is composite mixed, while stable lattice is realized, also have adjusted γ~
Ce2S3The absorption spectrum of pigment, so as to be allowed to still keep large red.It is low another object of the present invention is to provide above-mentioned nanoscale
The composite mixed type γ~Ce of valency ion2S3The preparation method of red pigment and its product obtained.
The purpose of the present invention is achieved by the following technical programs：
The composite mixed type γ~Ce of a kind of nanoscale low price ion provided by the invention2S3Red pigment, the Doped ions
The ionic valence condition of M is 2 and at least two kinds, according to molar ratio Ce3+∶MAlways=2 (1-x): 3x, wherein 0 ＜ x≤0.1.The present invention
Composite mixed low price ion enters γ~Ce2S3In lattice, by replacing Ce3+Ion and fill up present in lattice positive
Ionic vacancies and realize doping.
Further, Doped ions M of the present invention is Eu2+、Sm2+、Tm2+、Yb2+、Sr2+、Sn2+、Nd2+In at least two
Kind.The composite mixed type γ~Ce of ion2S3The granularity of red pigment is less than 500nm, red scale value a* >=32；In air gas
Still take on a red color appearance under atmosphere after 900 DEG C of temperature lower calcinations, red scale value a* >=30.
Another object of the present invention is achieved by the following technical programs：
The composite mixed type γ~Ce of above-mentioned nanoscale low price ion provided by the invention2S3The preparation method of red pigment, bag
Include following steps：
(1) solvent-thermal method prepares the sulphur cerium oxide precursor liquid suspension of the element containing Doped ions
By inorganic soluble cerium salt, at least two kinds of Doped ions inorganic soluble salt, sulphur source are dissolved in 60~80ml reactions and are situated between
Reaction system is formed in matter, wherein according to molar ratio sulphur source: total metal ion=1~2.5: 1, the dosage of reaction medium is 6
The total metal ions of~8L/mol, are reacted by solvent-thermal method, and the sulphur cerium oxide precursor body for obtaining the element containing Doped ions hangs
Supernatant liquid；
(2) the sulphur cerium oxide precursor body powder of the element containing Doped ions is prepared
The suspension is centrifuged, washes, alcohol is washed, dry after, be made the element containing Doped ions sulphur cerium oxide before
Drive body powder；
(3) the composite mixed type γ~Ce of ion2S3The preparation of red pigment
Additive, sintering aid are added in the sulphur cerium oxide precursor body powder, calcined after ground and mixed is uniform,
Cooling is to get to the composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment.
In said program, inorganic soluble cerium salt described in preparation method of the present invention is Ce (NO3)3·6H2O、CeCl3·
7H2O、Ce2(SO4)3·8H2O、Ce(Ac)3·nH2O；The Doped ions inorganic soluble salt is Eu2(SO4)3·H2O、
SmCl3·6H2O、Sm(NO3)3、Tm(NO3)3、Yb(NO3)3·5H2O、YbCl3、Sr(NO3)2、Sr(Ac)2、SrCl2、SnCl2·
2H2O、Nd(NO3)3、NdCl3In at least two kinds；The sulphur source is thiocarbamide, thioacetamide, tetraethylthiuram disulfide
(C10H20N2S4)；The reaction medium is ethylenediamine, ethylene glycol, ethyl alcohol.
Further, after reaction system stirs 30~180min in step (1) described in preparation method of the present invention, it is transferred to reaction
In kettle at a temperature of 150~300 DEG C reaction 6~for 24 hours.
Further, in step (3) described in preparation method of the present invention, the additive is sodium carbonate, potassium carbonate, carbonic acid
Calcium, magnesium carbonate, dosage are 2~3wt% of presoma powder；The sintering aid is diboron trioxide, and dosage is forerunner
2~3wt% of body powder.
Further, in step (3) described in preparation method of the present invention, the calcination stage is to be passed through indifferent gas at room temperature
Body Ar or N2, 300 DEG C are warming up to 5~10 DEG C/min；Then pass to CS2/ Ar mixed gas is warming up to 500 DEG C with 2 DEG C/min,
900 DEG C are warming up to 5 DEG C/min again, keeps the temperature 60~200min；The cooling stage is before being cooled to 300 DEG C, to be passed through CS2/Ar
Mixed gas, 300~200 DEG C are passed through Ar gas, and 200 DEG C~room temperature is not passed through atmosphere natural cooling.
The present invention utilizes the composite mixed type γ~Ce of above-mentioned nanoscale low price ion2S3The preparation method of red pigment is made
Product.
The invention has the advantages that：
(1) for the present invention in a manner that low price ion is composite mixed, part ion enters γ~Ce2S3Ce is replaced in lattice3+
Ion, and part ion has also filled up cation vacancy present in lattice, so as to effectively stabilize γ~Ce2S3Lattice, greatly
Width improves the high-temperature stability of pigment.
(2) low price ion of the invention is composite mixed, while stable lattice is realized, also has adjusted γ~Ce2S3Pigment
Absorption spectrum, color change caused by single doping is avoided, so as to be allowed to still keep large red.
(3) the composite mixed type γ~Ce of low price ion produced by the present invention2S3Red pigment granularity is less than 500nm, tinting strength, tinting power
By force, uniform particle sizes, good dispersion, red scale value a* >=32；Still take on a red color appearance after 900 DEG C of temperature calcinations in air atmosphere,
Red scale value a* >=30 are greatly expanded its application field under the high temperature conditions.
(4) for preparation method of the present invention without expensive equipment, simple for process easy to operate, influence factor is easy to control, and calcines
Temperature is low (only needing 900 DEG C), saves energy consumption, production cost is low, contributes to promotion and application.
Description of the drawings
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail：
Fig. 1 is the composite mixed type γ~Ce of low price ion made from the embodiment of the present invention one and embodiment two2S3Red pigment
X-ray diffraction spectrogram (XRD) (a be embodiment one, b be embodiment two)；
Fig. 2 is the composite mixed type γ~Ce of low price ion made from the embodiment of the present invention one2S3The scanning electron microscope of red pigment
(SEM) photo.
Specific embodiment
Embodiment one：
The composite mixed type γ~Ce of the present embodiment nanoscale low price ion2S3The preparation method of red pigment, step is such as
Under：
(1) solvent-thermal method prepares the sulphur cerium oxide precursor liquid suspension of the element containing Doped ions
By 3.50gCeCl3·7H2O、0.13gEu2(SO4)3·H2O、0.06gSnCl2·2H2O and 0.40g thiocarbamides are molten successively
In 70ml ethylenediamines, it is transferred to after being vigorously stirred 120min in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature
The lower reaction 12h of degree, obtains the sulphur cerium oxide precursor liquid suspension of Eu containing doped chemical, Sn；
(2) the sulphur cerium oxide precursor body powder of the element containing Doped ions is prepared
Above-mentioned suspension is centrifuged, washes, alcohol is washed, dry after, be made Eu containing doped chemical, Sn sulphur cerium oxide before
Drive body powder；
(3) the composite mixed type γ~Ce of ion2S3The preparation of red pigment
Sodium Carbonate Additive, sintering aid diboron trioxide, dosage are added in above-mentioned sulphur cerium oxide precursor body powder
Respectively 2.5wt%, 2.0wt% of presoma powder；It is calcined after ball milling mixing is uniform, i.e., is passed through inert gas at room temperature
Ar gas is warming up to 300 DEG C with 5 DEG C/min；Then pass to CS2/ Ar mixed gas is warming up to 500 DEG C with 2 DEG C/min, then with 5
DEG C/min is warming up to 900 DEG C, keep the temperature 180min；Then cooled down, that is, before being cooled to 300 DEG C, be passed through CS2/ Ar mixed gas,
300~200 DEG C are passed through Ar gas, and 200 DEG C~room temperature is not passed through atmosphere natural cooling；Wherein, CS2/ Ar mixed gas for Ar gas with
Bubbling mode is from equipped with CS2It is taken out of in the container of solution；Cooling, which finishes, obtains nanoscale low price ion Eu2+、Sn2+It is composite mixed
Type γ~Ce1.94Eu0.04Sn0.05S3Red pigment.
A in Fig. 1 is the X-ray diffraction spectrogram of pigment obtained by the present embodiment, and pigment is γ~Ce2S3
(PDF500851), Eu2+、Sn2+It is composite mixed not change the structure of cerium sulphide, but it is highly dispersed at Ce2S3In lattice.
Figure it is seen that pigment-dispersing obtained by the present embodiment is good, it is spherical, grain size 100nm.
Embodiment two：
The composite mixed type γ~Ce of the present embodiment nanoscale low price ion2S3The preparation method of red pigment, step is such as
Under：
(1) solvent-thermal method prepares the sulphur cerium oxide precursor liquid suspension of the element containing Doped ions
By 3.91gCe (NO3)3·6H2O、0.175gEu2(SO4)3·H2O、0.21gSmCl3·6H2O and 0.35g thiocarbamides according to
It is secondary to be dissolved in 70ml ethylene glycol, it is transferred to after being vigorously stirred 100min in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), 250
15h is reacted at a temperature of DEG C, obtains the sulphur cerium oxide precursor liquid suspension of Eu containing doped chemical, Sm；
(2) the sulphur cerium oxide precursor body powder of the element containing Doped ions is prepared
Above-mentioned suspension is centrifuged, washes, alcohol is washed, dry after, be made Eu containing doped chemical, Sm sulphur cerium oxide before
Drive body powder；
(3) the composite mixed type γ~Ce of ion2S3The preparation of red pigment
Additive magnesium carbonate, sintering aid diboron trioxide, dosage are added in above-mentioned sulphur cerium oxide precursor body powder
Respectively 3.0wt%, 2.5wt% of presoma powder；It is calcined after ball milling mixing is uniform, i.e., is passed through inert gas at room temperature
N2Gas is warming up to 300 DEG C with 8 DEG C/min；Then pass to CS2/ Ar mixed gas is warming up to 500 DEG C with 2 DEG C/min, then with 5 DEG C/
Min is warming up to 900 DEG C, keeps the temperature 180min；Then cooled down, that is, before being cooled to 300 DEG C, be passed through CS2/ Ar mixed gas, 300
~200 DEG C are passed through N2Gas, 200 DEG C~room temperature are not passed through atmosphere natural cooling；Wherein, CS2/ Ar mixed gas is Ar gas with bubbling
Mode is from equipped with CS2It is taken out of in the container of solution；Cooling, which finishes, obtains nanoscale low price ion Eu2+、Sm2+Composite mixed type γ
~Ce1.88Eu0.06Sm0.12S3Red pigment.
B in Fig. 1 is the X-ray diffraction spectrogram of pigment obtained by the present embodiment, and pigment is γ~Ce2S3
(PDF500851), Eu2+、Sm2+It is composite mixed not change the structure of cerium sulphide, but it is highly dispersed at Ce2S3In lattice.
Embodiment three：
The composite mixed type γ~Ce of the present embodiment nanoscale low price ion2S3The preparation method of red pigment, with embodiment one
The difference is that：
Sulphur source in the present embodiment step (1) is tetraethylthiuram disulfide (C10H20N2S4), dosage 1.5g；Step
(2) additive is calcium carbonate in, and dosage is the 3.0wt% of presoma powder, before the dosage of sintering aid diboron trioxide is
Drive the 3.0wt% of body powder.
Example IV：
The composite mixed type γ~Ce of the present embodiment nanoscale low price ion2S3The preparation method of red pigment, with embodiment one
The difference is that：
Raw material is 4.10gCeCl in the present embodiment step (1)3·7H2O、0.321gYb(NO3)3·5H2O、0.128g
NdCl3, 1.50g tetraethylthiuram disulfides (C10H20N2S4)；Additive is magnesium carbonate in step (2), and dosage is forerunner
The 3.0wt% of body powder, the dosage of sintering aid diboron trioxide are the 3.0wt% of presoma powder.Obtained pigment is to receive
Meter level low price ion Yb2+、Nd2+Composite mixed type γ~Ce1.84Yb0.14Nd0.1S3Red pigment.
Embodiment five：
The composite mixed type γ~Ce of the present embodiment nanoscale low price ion2S3The preparation method of red pigment, with embodiment two
The difference is that：
Sulphur source in the present embodiment step (1) is tetraethylthiuram disulfide (C10H20N2S4), dosage 1.5g；Step
(2) additive is calcium carbonate in, and the dosage of sintering aid diboron trioxide is the 3.0wt% of presoma powder.
Performance test：
The composite mixed type γ~Ce of ion obtained by the embodiment of the present invention2S3Red pigment is had using Hangzhou Yan Te science and technology
The full-automatic chromascopes of YT-ACM402 of limit company production are tested：The illumination of D65 working flares is simulated, it is several using d/0 illuminating watches
What condition diffuses bulb diameter 150mm, a diameter of 30mm of instrument connection, and test wavelength scope is visible ray (400~700nm), is measured
By black (0) to white (100), a* is represented by green (-) to red (+), b* for pigment color parameter CIE-L*a*b*, wherein L* representative
It represents by blue (-) to yellow (+).Measured pigment chromatic value is as shown in table 1.
The composite mixed type γ~Ce of ion obtained by 1 various embodiments of the present invention of table2S3The chromatic value of red pigment
| Embodiment | L* | a* | b* |
| Embodiment one | 31.38 | 32.46 | 26.43 |
| Embodiment two | 31.42 | 32.38 | 25.39 |
| Embodiment three | 31.48 | 33.40 | 25.87 |
| Example IV | 31.35 | 32.48 | 25.43 |
| Embodiment five | 31.52 | 32.42 | 25.46 |
With the commercial γ~Ce not wrapped up2S3Colorant is as a comparison case.Comparative example γ~Ce2S3Colorant and the present invention
The composite mixed type γ~Ce of ion obtained by embodiment one2S3Red pigment, the chromatic value such as table 2 after being calcined in air atmosphere
It is shown.
2 embodiment of the present invention one of table and comparative example calcined in air atmosphere after chromatic value
Claims (10)
1. a kind of composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment, it is characterised in that：The Doped ions M's
Ionic valence condition is 2 and at least two kinds, according to molar ratio Ce3+∶MAlways=2 (1-x): 3x, wherein 0 ＜ x≤0.1.
2. the composite mixed type γ~Ce of nanoscale low price ion according to claim 12S3Red pigment, it is characterised in that：
The Doped ions M is Eu2+、Sm2+、Tm2+、Yb2+、Sr2+、Sn2+、Nd2+In at least two kinds.
3. the composite mixed type γ~Ce of nanoscale low price ion according to claim 12S3Red pigment, it is characterised in that：
The composite mixed type γ~Ce of ion2S3The granularity of red pigment is less than 500nm.
4. the composite mixed type γ~Ce of nanoscale low price ion according to claim 1 or 2 or 32S3Red pigment, it is special
Sign is：The composite mixed type γ~Ce of ion2S3Red scale value a* >=32 of red pigment；In air atmosphere in 900 DEG C of temperature
Still take on a red color appearance after the lower calcining of degree, red scale value a* >=30.
5. the composite mixed type γ~Ce of one of the claim 1-4 nanoscale low price ions2S3The preparation method of red pigment,
It is characterized by comprising following steps：
(1) solvent-thermal method prepares the sulphur cerium oxide precursor liquid suspension of the element containing Doped ions
By inorganic soluble cerium salt, at least two kinds of Doped ions inorganic soluble salt, sulphur sources are dissolved in 60~80ml reaction mediums
And reaction system is formed, and wherein according to molar ratio sulphur source: total metal ion=1~2.5: 1, the dosage of reaction medium is 6~8L/
The total metal ions of mol, are reacted by solvent-thermal method, obtain the sulphur cerium oxide precursor liquid suspension of the element containing Doped ions；
(2) the sulphur cerium oxide precursor body powder of the element containing Doped ions is prepared
The suspension is centrifuged, washes, alcohol is washed, dry after, be made the element containing Doped ions sulphur cerium oxide precursor body
Powder；
(3) the composite mixed type γ~Ce of ion2S3The preparation of red pigment
Additive, sintering aid are added in the sulphur cerium oxide precursor body powder, is calcined after ground and mixed is uniform, is cold
But to get to the composite mixed type γ~Ce of nanoscale low price ion2S3Red pigment.
6. the composite mixed type γ~Ce of nanoscale low price ion according to claim 52S3The preparation method of red pigment,
It is characterized in that：The inorganic soluble cerium salt is Ce (NO3)3·6H2O、CeCl3·7H2O、Ce2(SO4)3·8H2O、Ce
(Ac)3·nH2O；The Doped ions inorganic soluble salt is Eu2(SO4)3·H2O、SmCl3·6H2O、Sm(NO3)3、Tm
(NO3)3、Yb(NO3)3·5H2O、YbCl3、Sr(NO3)2、Sr(Ac)2、SrCl2、SnCl2·2H2O、Nd(NO3)3、NdCl3In
At least two kinds；The sulphur source is thiocarbamide, thioacetamide, tetraethylthiuram disulfide；The reaction medium is ethylenediamine, second
Glycol, ethyl alcohol.
7. the composite mixed type γ~Ce of nanoscale low price ion according to claim 52S3The preparation method of red pigment,
It is characterized in that：After reaction system stirs 30~180min in the step (1), it is transferred in reaction kettle in 150~300 DEG C of temperature
Lower reaction 6~for 24 hours.
8. the composite mixed type γ~Ce of nanoscale low price ion according to claim 52S3The preparation method of red pigment,
It is characterized in that：In the step (3), the additive is sodium carbonate, potassium carbonate, calcium carbonate, magnesium carbonate, and dosage is forerunner
2~3wt% of body powder；The sintering aid is diboron trioxide, and dosage is 2~3wt% of presoma powder.
9. the composite mixed type γ~Ce of nanoscale low price ion according to claim 5 or 82S3The preparation side of red pigment
Method, it is characterised in that：In the step (3), the calcination stage is to be passed through inert gas Ar or N at room temperature2, with 5~10
DEG C/min is warming up to 300 DEG C；Then pass to CS2/ Ar mixed gas is warming up to 500 DEG C with 2 DEG C/min, then is heated up with 5 DEG C/min
To 900 DEG C, 60~200min is kept the temperature；The cooling stage is before being cooled to 300 DEG C, to be passed through CS2/ Ar mixed gas, 300~
200 DEG C are passed through Ar gas, and 200 DEG C~room temperature is not passed through atmosphere natural cooling.
10. utilize one of the claim 5-9 composite mixed type γ~Ce of the nanoscale low price ion2S3The preparation of red pigment
Product made from method.
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| CN114084898A (en) * | 2021-12-06 | 2022-02-25 | 景德镇陶瓷大学 | High-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114084898A (en) * | 2021-12-06 | 2022-02-25 | 景德镇陶瓷大学 | High-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method |
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